Supercritical Fluid Extraction of Mycotoxins from Feeds with Analysis by Lc/Uv and Lc/Ms

Abstract

The use of supercritical fluid extraction with supercritical carbon dioxide and a matrix modifier is described for the isolation of three trichothecene mycotoxins from yellow corn meal and rolled oats. The quantity of supercritical carbon dioxide used in each extraction was 30 mL which contained 5% methanol used as a modifier. The pressure was maintained at 550 atm., and the temperature of the extraction chamber was set at 60 degrees. Recovery of the target analytes from cereal and corn feed by supercritical fluid extraction (SFE) varied from 85 to 95 % depending on the target compound. The mycotoxins, deoxynivalenol (DON), deacetoxyscirpenol (DAS) and T-2 toxin (T-2) were monitored in the SFE extracts by high performance liquid chromatography with UV-detection (HPLC-UV) or ion spray mass spectrometry under full-scan, selected ion monitoring (SIM) and selected reaction monitoring (SRM) modes. There are significant restrictions in the HPLC-UV detection limits for T-2 and DAS, in particular, due to their low UV absorbance. With HPLC-UV and also HPLC-MS in the full-scan mode of acquisition the considerable interference from co-eluting fat-soluble compounds precluded detection of these compounds in feed extracts. In the SIM and SRM LC/MS modes the target analytes could be readily detected at the 250 ppb level in the cereal SFE matrix extracts.